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#$Date: 2023-05-10 01:51:12 +0300 (Wed, 10 May 2023) $
#$Revision: 283634 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712986.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712986
loop_
_publ_author_name
'Khrizanforova, Vera'
'Fayzullin, Robert R.'
'Bogomyakov, Artem'
'Morozov, Vladimir'
'Batulin, Ruslan Germanovich'
'Gerasimova, Tatiana'
'Islamov, Daut'
'Budnikova, Yulia H.'
_publ_section_title
;
 Cobalt(II) coordination to N4-acenaphthene-based ligand and its sodium
 complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00347G
_journal_year                    2023
_chemical_formula_moiety         'C24 H14 N4'
_chemical_formula_sum            'C24 H14 N4'
_chemical_formula_weight         358.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9641(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2713(5)
_cell_length_b                   13.6010(3)
_cell_length_c                   7.2095(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.58
_cell_measurement_theta_min      2.37
_cell_volume                     1683.95(8)
_computing_cell_refinement       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_reduction        'APEX4 v2021.10-0 (Bruker AXS)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            80644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.589
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9376
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group 2/m for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.000   0.003
 Restraint esd for equal adjacent scale factors =  0.0060
 Maximum odd and even orders for spherical harmonics =   1   4
 wR2(int) =  0.1526 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0477 (selected reflections only, after parameter refinement)

   82768 total and   4178 unique reflections assuming Friedel's law
 plus   8945 total and  1561 unique reflections in fast scans
 Reflections rejected for which |I-|/su >   3.00
   82180 total and   4178 unique reflections left after |I-|/su test
 plus   8823 total and  1560 unique reflections in fast scans

 Error model 5: refine all K and overall g
 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  27.2  0.0299  0.223 - 0.463  0.993 - 1.023  1.006  0.0260  38.5    6382    5445
   2  27.2  0.0345  0.378 - 0.845  0.993 - 1.016  1.030  0.0260  38.5    6508    5402
   3  27.2  0.0266  0.303 - 0.498  0.993 - 1.021  0.970  0.0260  38.5    6433    5518
   4  27.2  0.0326  0.350 - 0.700  0.993 - 1.019  0.995  0.0260  38.5    6424    5430
   5  27.2  0.0266  0.298 - 0.420  0.993 - 1.024  0.967  0.0260  38.5    6395    5510
   6  27.2  0.0296  0.327 - 0.739  0.995 - 1.021  0.984  0.0260  38.5    6462    5432
   7 -27.2  0.0288  0.342 - 0.673  0.993 - 1.021  0.965  0.0260  38.5    6220    5269
   8  27.2  0.0314  0.366 - 0.910  0.993 - 1.020  0.964  0.0260  38.5    6498    5421
   9  27.2  0.0266  0.268 - 0.456  0.993 - 1.023  0.944  0.0260  38.5    6435    5546
  10  27.2  0.0281  0.223 - 0.435  0.993 - 1.017  0.988  0.0260  38.5    6331    5439
  11  27.2  0.0302  0.322 - 0.494  0.993 - 1.024  1.017  0.0260  38.5    4908    4278
  12  27.2  0.0278  0.299 - 0.433  0.994 - 1.023  0.987  0.0260  38.5    4384    3826
  13  27.2  0.0284  0.324 - 0.621  0.993 - 1.020  0.959  0.0260  38.5    6445    5475
  14   0.0  0.0301  0.330 - 0.723  0.993 - 1.019  1.177  0.0260  38.5    2355    2085
  15f  0.0  0.0549  0.322 - 0.785  0.993 - 1.021  1.097  0.0260  38.5    4589    3254
  16f  0.0  0.1181  2.779 - 4.359  0.995 - 1.016  0.944  0.0260  38.5    4234    2272

      63 Overloads replaced by fast scan measurements
   82243 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.9376  0.9754
 Additional spherical absorption correction applied with mu*r =  0.0142
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method 'a DCM solution at r.t.'
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0637P)²+0.6356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3751
_reflns_number_total             4057
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz006
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7712986
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.988
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.58172(3) 0.64024(3) 0.29158(7) 0.01382(9) Uani 1 1 d . . . . .
N2 N 0.55385(3) 0.88775(4) 0.14420(7) 0.01491(9) Uani 1 1 d . . . . .
C11 C 0.54121(3) 0.55806(4) 0.27341(8) 0.01337(9) Uani 1 1 d . . . . .
C12 C 0.56797(3) 0.45553(4) 0.28933(8) 0.01427(10) Uani 1 1 d . . . . .
C13 C 0.63856(3) 0.40910(4) 0.32872(9) 0.01718(11) Uani 1 1 d . . . . .
H13 H 0.685216 0.445966 0.355749 0.021 Uiso 1 1 calc R U . . .
C14 C 0.63996(4) 0.30469(5) 0.32796(10) 0.01925(11) Uani 1 1 d . . . . .
H14 H 0.688532 0.272246 0.354784 0.023 Uiso 1 1 calc R U . . .
C15 C 0.57344(4) 0.24846(4) 0.28974(9) 0.01884(11) Uani 1 1 d . . . . .
H15 H 0.576836 0.178756 0.290041 0.023 Uiso 1 1 calc R U . . .
C16 C 0.500000 0.29479(6) 0.250000 0.01604(13) Uani 1 2 d S T P . .
C17 C 0.500000 0.39769(6) 0.250000 0.01427(12) Uani 1 2 d S T P . .
C18 C 0.54041(3) 0.72491(4) 0.26664(8) 0.01297(9) Uani 1 1 d . . . . .
C21 C 0.58691(3) 0.81487(4) 0.27075(8) 0.01309(9) Uani 1 1 d . . . . .
C22 C 0.66413(3) 0.81805(4) 0.39781(9) 0.01545(10) Uani 1 1 d . . . . .
H22 H 0.685593 0.764921 0.484953 0.019 Uiso 1 1 calc R U . . .
C23 C 0.70907(3) 0.89987(4) 0.39506(9) 0.01690(10) Uani 1 1 d . . . . .
H23 H 0.762035 0.903352 0.478378 0.020 Uiso 1 1 calc R U . . .
C24 C 0.67494(3) 0.97653(4) 0.26786(9) 0.01745(11) Uani 1 1 d . . . . .
H24 H 0.703698 1.034281 0.264393 0.021 Uiso 1 1 calc R U . . .
C25 C 0.59756(3) 0.96698(4) 0.14528(9) 0.01645(10) Uani 1 1 d . . . . .
H25 H 0.574594 1.019459 0.057828 0.020 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 N1 C18 115.95(5) . . ?
C25 N2 C21 117.44(5) . . ?
N1 C11 C11 122.25(3) . 2_655 ?
N1 C11 C12 129.38(5) . . ?
C11 C11 C12 108.35(3) 2_655 . ?
C13 C12 C17 118.89(5) . . ?
C13 C12 C11 135.67(5) . . ?
C17 C12 C11 105.44(5) . . ?
C12 C13 C14 118.35(5) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 122.58(5) . . ?
C15 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
C14 C15 C16 120.05(6) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 116.34(4) . 2_655 ?
C17 C16 C15 116.34(4) . . ?
C15 C16 C15 127.32(8) 2_655 . ?
C16 C17 C12 123.79(3) . 2_655 ?
C16 C17 C12 123.79(3) . . ?
C12 C17 C12 112.42(7) 2_655 . ?
N1 C18 C18 121.68(3) . 2_655 ?
N1 C18 C21 114.13(5) . . ?
C18 C18 C21 124.16(3) 2_655 . ?
N2 C21 C22 122.84(5) . . ?
N2 C21 C18 118.25(5) . . ?
C22 C21 C18 118.82(5) . . ?
C23 C22 C21 119.08(5) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 118.52(5) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C23 C24 C25 118.58(5) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N2 C25 C24 123.52(5) . . ?
N2 C25 H25 118.2 . . ?
C24 C25 H25 118.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C11 1.3223(7) . ?
N1 C18 1.3549(7) . ?
N2 C25 1.3396(7) . ?
N2 C21 1.3430(7) . ?
C11 C11 1.4263(11) 2_655 ?
C11 C12 1.4692(7) . ?
C12 C13 1.3758(8) . ?
C12 C17 1.4147(7) . ?
C13 C14 1.4204(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.3818(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.4204(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.3994(11) . ?
C18 C18 1.4127(10) 2_655 ?
C18 C21 1.4841(7) . ?
C21 C22 1.3960(8) . ?
C22 C23 1.3872(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.3880(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.3942(9) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 N1 C11 C11 1.18(9) . . . 2_655 ?
C18 N1 C11 C12 179.26(5) . . . . ?
N1 C11 C12 C13 1.26(11) . . . . ?
C11 C11 C12 C13 179.56(7) 2_655 . . . ?
N1 C11 C12 C17 -177.95(5) . . . . ?
C11 C11 C12 C17 0.34(7) 2_655 . . . ?
C17 C12 C13 C14 0.04(8) . . . . ?
C11 C12 C13 C14 -179.10(6) . . . . ?
C12 C13 C14 C15 -0.13(9) . . . . ?
C13 C14 C15 C16 -0.29(9) . . . . ?
C14 C15 C16 C17 0.76(6) . . . . ?
C14 C15 C16 C15 -179.24(6) . . . 2_655 ?
C15 C16 C17 C12 -0.89(4) 2_655 . . 2_655 ?
C15 C16 C17 C12 179.11(4) . . . 2_655 ?
C15 C16 C17 C12 179.11(4) 2_655 . . . ?
C15 C16 C17 C12 -0.89(4) . . . . ?
C13 C12 C17 C16 0.50(6) . . . . ?
C11 C12 C17 C16 179.87(3) . . . . ?
C13 C12 C17 C12 -179.50(6) . . . 2_655 ?
C11 C12 C17 C12 -0.13(3) . . . 2_655 ?
C11 N1 C18 C18 3.13(9) . . . 2_655 ?
C11 N1 C18 C21 -174.89(5) . . . . ?
C25 N2 C21 C22 -1.30(8) . . . . ?
C25 N2 C21 C18 -177.77(5) . . . . ?
N1 C18 C21 N2 141.03(5) . . . . ?
C18 C18 C21 N2 -36.93(9) 2_655 . . . ?
N1 C18 C21 C22 -35.58(7) . . . . ?
C18 C18 C21 C22 146.46(7) 2_655 . . . ?
N2 C21 C22 C23 0.29(9) . . . . ?
C18 C21 C22 C23 176.74(5) . . . . ?
C21 C22 C23 C24 1.11(9) . . . . ?
C22 C23 C24 C25 -1.45(9) . . . . ?
C21 N2 C25 C24 0.93(9) . . . . ?
C23 C24 C25 N2 0.44(9) . . . . ?
